干旱区生态环境知识资源中心(Arid): Mixed-mode solid phase extraction combined with LC-MS/MS for determination of empagliflozin and linagliptin in human plasma

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DOI	10.1016/j.microc.2018.11.015
	Mixed-mode solid phase extraction combined with LC-MS/MS for determination of empagliflozin and linagliptin in human plasma
	Shah, Priyanka A.; Shrivastav, Pranav S.; George, Archana
通讯作者	Shrivastav, Pranav S.
来源期刊	MICROCHEMICAL JOURNAL
ISSN	0026-265X
EISSN	1095-9149
出版年	2019
卷号	145 页码:523-531
英文摘要	A selective, sensitive, precise and accurate liquid chromatography-tandem mass spectrometry method was developed and validated for the concurrent determination of antidiabetic drugs, empagliflozin and linagliptin in human plasma. Sample preparation was tested on several reversed-phase solid-phase extraction (SPE) sorbents with different chemistries like hydrophilic-lipophilic balance (Oasis HLB), mixed-mode cation exchange (Oasis MCX) and weak-cation exchange (Oasis WCX). SPE conditions like sample pH, washing and elution solvents were suitably optimized. Best results were obtained using Oasis MCX cartridges in terms of extraction recovery (78-88%) and matrix effects (similar to 3.0%) for both the analytes. Chromatographic conditions for the separation of analytes and their labeled internal standards (ISs) were established on XSelect HSS Cyano (50 x 2.1 mm, 3.5 mu m) column using 2 mM ammonium acetate buffer and acetonitrile as the mobile phase. Detection of analytes was achieved using electrospray ionization in the positive mode. For quantitative analysis, multiple reaction monitoring transitions were m/z 451.3 -> 71.1 for empagliflozin and m/z 473.2 -> 420.2 for linagliptin. Standard curve concentrations were validated in the range of 1.50-1500 ng/mL for empagliflozin and 0.015-15.0 ng/mL for linagliptin. The infra-batch and inter-batch precision (% CV) was < 3.7 for both the drugs. The stability of the analytes established under different storage conditions was found to be appropriate for routine laboratory practices. The validated method was used to study the pharmacokinetics of the drugs using a single oral dose of fixed-dose combination tablet consisting of 25 mg empagliflozin and 5 mg linagliptin in healthy subjects.
英文关键词	Empagliflozin Linagliptin Mixed-mode solid phase extraction Human plasma LC-MS/MS Pharmacokinetics
类型	Article
语种	英语
国家	India
收录类别	SCI-E
WOS记录号	WOS:000457513000069
WOS关键词	MASS-SPECTROMETRY METHOD ; COMBINATION THERAPY ; TYPE-2 ; METFORMIN ; PHARMACOKINETICS ; INHIBITOR
WOS类目	Chemistry, Analytical
WOS研究方向	Chemistry
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/217606
作者单位	Gujarat Univ, Sch Sci, Dept Chem, Ahmadabad 380009, Gujarat, India
推荐引用方式 GB/T 7714	Shah, Priyanka A.,Shrivastav, Pranav S.,George, Archana. Mixed-mode solid phase extraction combined with LC-MS/MS for determination of empagliflozin and linagliptin in human plasma[J],2019,145:523-531.
APA	Shah, Priyanka A.,Shrivastav, Pranav S.,&George, Archana.(2019).Mixed-mode solid phase extraction combined with LC-MS/MS for determination of empagliflozin and linagliptin in human plasma.MICROCHEMICAL JOURNAL,145,523-531.
MLA	Shah, Priyanka A.,et al."Mixed-mode solid phase extraction combined with LC-MS/MS for determination of empagliflozin and linagliptin in human plasma".MICROCHEMICAL JOURNAL 145(2019):523-531.